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H. 8111111881188 8 E. BLUM. APPARATUS FOR D'ISTILLING AMMONIA.

No. 858,198. Patented 1188.22, 1887.

N. vergis. mmgmugmphur. washington D. c.

I (No Model.) 3 Sheets-Sheet 2.

H. GRNEBERG & E. BLUM. APPARATUS FOR DISTILLING AMMONIA.

3 Sheets-Sheet 3.

(No Model.)

, H GRUNBBERG & E BLUM APPARATUS PoR DISTILLING AMMONIA. No. 358,196.

Patented Feb. 22, 1887.

UNITED STATES PATENT OFFICE.

HERMANN GRNEBERG, OF COLOGNE, AND EMIL BLUM, OF BERLIN, GER- MANY, ASSIGNORS OF ONE-THIRD TO HENRY SIMON, OF MANCHESTER,

ENGLAND.

APPARATUS Fon DISTILLING AMMONIA.

SPECIFICATION forming part of Letters Patent No. 358,196, dated February 22, 1887.

Application tiled April 9, 1886. Serial No. 198,385. (No model.) Patentedin Germany February 11, 1885, No. 33,320; in England February 25, 1885, No. 2,578; in France April 11,1885, No. 168,211; in Austria-Hungary April 18, 1885, No. 14,324, and in Italy April 14, 1885, XIX, 18,801. f

.To all whom it may concern.-

Be it known that we, HERMANN GRNE BERG and EMIL BLUM, subjects of the Emperor of Germany, residing, respectively, at

Cologne, in the German Empire, and Berlin, in the German Empire, have invented new and useful Improved Apparatus for the Dis tillation of Ammonia fromy Ammoniacal Liquors and forthe Treatment ofthe Resulting Am- Io moniacal Vapors, (for which We have obtained Letters Patent in Germany, February 1l, 1885, No. 33,320; Great Britain, February 25, 1885, No. 2,578; France, April 11,1885, No. 168,211; AuStriaHungary, A pril 13, 1885, No. 14,324,

and Italy Apri-l 14, 1885, Vol. XIX, No. 118.201,) of which the following is a specilicat ion.l

This invention relates to apparatusfor distilling and concentrating ammoniacal liquors 2o in a continuous manner, wherein such liquors are caused to pass downward through a col umn wherein, as they iiow successively from one tray to the next below, they are brought into intimate contact with steam passing in a 2 5 contrary direction, whereby the steam is made to liberate the ammonia from the liquor, the

latter being then made to flow into a chamberco'ntaining milk oflime, whereby any ammonia remaining in-a combined state is rendered 3o free. The ammoniacal vapors and steam that issue from the top of the still are lirst made to pass into a vessel, where they are brought in contact with the ammoniacal liquor before it passes into the still, so that on the one hand 3 5 this liquor becomes heated preparatory to its distillation, while on the other hand, the ammomia-vapors become cooled. These are then conducted into one or other of two vessels charged with milk of lime, in order "to free 4o them from carbonio acid and other impurities, the said vesselsv being so 'arranged that while the ammonia-vapor is passing through the one the contents of the other, which have previously had the ammoniavapor passed through them, are first treated with steam, in order to drive off the 'ammonia taken up by the lime-Water, and are then discharged, after which the vessel is charged with a fresh supply of milk of lime. The ammonia-vapor isa .concentrating-vessel for the production of concentrated ammoniacal liquor, or into apparat-us for the production of either sal ammoniac or sulphate of ammonia.

We will proceed to describe the above-mentioned improved apparatus in connection with the accompanying drawings, in which Figure 1 shows a diagram elevation, partly in section, of the entire apparatus. Fig. 2 shows a plan, and Fig. 3shows a sectional elevation, of the still. Fig. 4 shows a cross-section ofthe same atx w. Fig. 3. Figs. 5 and 6 show modified constructionsof the bottom part of the still. Fig. 7 shows a modified construction of the combined heater and cooler. Fig. 8 shows the concentratingvessel for the au1- monia-vapor, and Fig. 9 shows a modified construction of the linie-vessels.

' The still 'consists of the Well-known arrangement of a column, A, in which the ammoniacal liquor is caused to flow downward succes sively through a number of trays, while steam is caused to iiow upward in intimate contact with liquor, so as to liberate the ammoniaeal vap or therefrom. Arrived at the bottom tray, b, more or less deprived of its ammonia, the liquor flows through the pipe cinto the chamber d, containing milk of lime, so that by miX- ing with this any ammonia remaining in the liquor in a combined state isy rendered free. The liquor, after treatment with the milk of lime, which is continuously fed into the chamber, overflows through the pipe e and descends into a well, f, in a second chamber, F. ln this well any solid suspended matter becomes deposited, while the liquor overdows its edge onto the stepped surface T, consisting of a series ot' circular steps of increasing diameter,

so that the liquorvin flowing down over them centric annular partitions I to pass upward in intimate contact with the liquid flowing down over the steps, so as to take up what free ammonia is still contained therein. Arrived at the top of the steps, the mixed steam and ammonia-vapor passes into the upper chamber, d, through tubes 7:, situated eoncentrically within other tubes, Z, closed at their upper ends and open at the lower ends, so that the mixed steam and vapor, after rising through the tubes k, has to descend again through l and issue iu a nely-divided state into the mixture ot' milk of lime and liquor contained in the chamber. The steam is thus caused to disengage a further quantity of ammonia from the liquor,and then passes up through thetower A in the wellknown manner, iinallyissuingat top, together with the ammonia-vapor, through the pipe a. The deposit in the well fis discharged from time to time through the discharge-valvej, operated by the lever f f.

Instead of constructing the stepped surface T as shown at Fig. 3, it may consist of a number of concentric rings of graduated height, as shown in section at Fig. 5. It may also be made of polygonal or segmental form instead of circular; also, in place of the annular partitions I, the casing of the apparatus may be formed inclined, as shown in the modification at Fig. 6, so as to cause the steam to pass in close contact with the liquid.

The pipe a conducts the mixed steam and ammoniacal vapor into a vessel, B, into which the ammoniacal liquor that is to be fed into the still is also caused to enter through a pipe, m, opening into the same box, m', into which the mixed steam and ammoniacal vapors pass, so that the liquor and vapor are brought into intimate contact and issue together through the pipe m2 into B, where the vapor is made to bubble up through the liquor on its way to the pipe o. rlhe ammonia-vapor thus becomes effectually cooled, while at the same time the liquor becomes heated before ilowing off through the bent pipe a into the still. Fig. 7 shows a modified arrangement of the abovedescribed combined heater and cooler, wherein the upper part of the vessel B contains a coil, B', through which cold water is made to ilow, entering at B2 and issuing at B, into a tank, B, surrounding B, whence it overflows through a pipe, By this means the am monia-vapor contained in the upper part of the vessel B is still further cooled before issuing through o. The cooled ammoniacal vapor is conducted from the vessel B through the pipe 0 to the one or other of the two vessels C C2. containing milk of lime, through which the vapor is made to pass so as to free it from any carbonio acid, &c. For this purpose the pipe ois provided with two branches, o o, leading, respectively, into the vessels C C2, in which they descend to near the bottom, where they are perforated, so as to allow the ammoniavapor to issue in divided streams into the linie-liquid. Each branch pipe is provided with a stopcoek, l and 3, so that while the ammoniafvapor is being admitted into the one vessel the communication with the other one can be cut off. From the tops of the Vessels C C2 other pipes, p, also provided with stopcocks 2 and 4, pass either to a cooling apparatus, D, for the production of concentrated ammoniacal liquor, or with the necessary apparatus of known construction for the production of either sal ammoniac or sulphate of ammonia. 4

The construction of the vessel D is shown more clearly in the enlarged elevation at Fig. 8. It consists of'a casing, D, within which is a vessel, t', into which passes the pipe p from the lime-vessels, and which contains a coil, j, for the circulation of cold water, entering at top through the pipe q and issuing atbottom j into the casing D, whence it passes away at r. The ammoniacal vapor, entering the Vessel fi from the pipe p and becoming refrigerated and condensed by contact with the eoilj, flows oil' through the bent pipe s.

s is a cock for the discharge, from time to time, of accumulated oily impurities floating on the ammonialiquor.

XVhen the milk of lime in the one vesselsay C-has become spent by the passage of ammoniacal vapor through it, the cocks l and 2 are, closed and 3 and et are opened, so that the ammoniacal vapor will now pass from o into C2 and thence to the cooler D. A steampipe, g, provided with branches and stop-cocks, communicates with the pipes o o2 of the vessels G C2, so that after C has been cnt off from thc supply-pipe o steam is admitted into the milk of lime, so as to drive off any ammonia taken up thereby, the resulting mixture of ammoniacal vapor and steam being led back into the still A through a pipe c, also provided with stop-cocks. rlhe spent lime-liquor is then discharged from C through the discharge-cock 5, and a fresh charge of milk of lime having been introduced through the pipe a', G is again putin communication with o and D, and the communications of C2 are closed so soon as the contents hereofhave become spent. Thus the continuous operation of the still and the purifying and condensing apparatus is maintained.

Fig. 9 shows a vertical section of a somewhat modiiicd form of the vessels C' C2, in which these are provided with stirring apparatus consisting of revolving inclined vanes situated immediately below the orifice of the pipe o', through which the ammoniacal vapor enters, so that an intimate admixtnre of the latter in a iinely-divided state with the milk of lime is insured. The shaft t of the 'vanes passes up through the pipe o and is rotated through gearing by any convenient motor.

Having thus described the nature of our invention and the best means we know for carrying the same into practical effect,we claim- 1. In combination with apparatus for dis- ICO IIO

tilling ammonia from ammoniacal liquor, a chamber containing a stepped surface onto which the limeliquor charged with ammoniacal vapor flows from the lime-chamber above, the liquor on owing down in a thin stream over the stepped surface being subjected to intimate contact with steam, whereby the ammonia is disengaged therefrom and carried back into the lime-chamber, substantially as herein described.

2.l In combination with a stepped surface over which the liquor containing ammonia descending from the ammonia-still is made to flow, a well or pocket into which the liquor flows from the lime-chamber before passing on to the stepped surface, in order to separate solid suspended matter therefrom, substantially as herein described.

3. The combination, with a stepped surface over which the liquor containing ammonia descending from the ammonia-still is made to flow, of annular partitions or equivalent appliances for causing the stream to come in contact with the liquor flowing over the steps, substantially as herein described.

4. Apparat-us for treating ammonia-vapor passing from the ammonia-still with milk of lime, consisting of two closed vessels having each, first, a pipe branching from thepipe conveying the ammonia-vapor from the still and provided with a stop-cock; secondly, a steam-supply pipe communicating with the said branch pipes and also provided with a stopcock; thirdly, another branch pipe provided with a stopcock communicating with a' pipe for conveying the ammonia-vapor to the condensing-vessel or other apparatus; fourthly, a branch pipe provided with a stop-cock communicating with a pipe for conveying the ammonia-vapor liberated by the action of the steam back into the still, fthly, a pipe for `jacket for the circulation of cold water and containing a coil of pipes through which the cold water is made to iiow before entering the jacket, the ammonia-vapor being led into the top of the vessel by a'pipe, so as to become condensed by contact with the coil-r and the cooled sides of the vessel, the resulting concentrated ammonia water being led away through a Siphon-bend, substantially as herein described.

In testimony whereof we have signed our naines to this specification, in the presence of two subscribing witnesses, the 8th and 12th days of March, A. D. 1886.

HERMANN GRUNEBERG. EMIL BLUM. Witnesses as to the signature of Hermann Griineberg:

E. WEYRACK, Jos: RAWE. Witnesses Aas to the signature of Emil Blum:

B. Roi, M. W. MOORE. 

